• Title/Summary/Keyword: solvent ratio

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Oxidative Desulfurization of Marine Diesel Using WOx/SBA-15 Catalyst and Hydrogen Peroxide (WOx/SBA-15 촉매와 과산화수소를 이용한 선박용 경유의 산화 탈황 연구)

  • Oh, Hyeonwoo;Kim, Ji Man;Huh, Kwang-Sun;Woo, Hee Chul
    • Korean Chemical Engineering Research
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    • v.55 no.4
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    • pp.567-573
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    • 2017
  • In this work, tungsten oxide ($WO_x$) supported on SBA-15 (mesoporous silica) were prepared and applied for oxidative desulfurization of sulfur compounds in marine diesel containing about 230 ppmw of sulfur concentration. Prepared catalysts were examined by two steps; at first step, oxidation reaction carried out with hydrogen peroxide as oxidant and then the oxidized sulfur compounds were extracted by acetonitrile as solvent. Catalysts were characterized by using X-ray diffraction, X-ray fluorescence, X-ray photoelectron spectroscopy and $N_2$ adsorption-desorption isotherms. Tungsten oxide exists as monoclinic crystal system on SBA-15 and over about 10 wt% of the $WO_x$ loading took the form of multi-layers on SBA-15. The 13 wt% $WO_x$/SBA-15 catalyst exhibite highest activity, achieving about 76.3% sulfur removal in the reaction conditions, such as catalyst amount of 0.1 g, reaction temperature at $90^{\circ}C$, reaction time for 3 h and O/S molar ratio of 10. One time oxidation reaction is enough oxidize the sulfur compounds in marine diesel completely. The repetition experiment of extraction process indicated that sulfur removal could reach 94.4% after 5 times.

Synthesis and Properties of Copolyester Resin for Precoated MeTAL (Precoated Metal용 Copolyester Resin의 합성 및 물성)

  • Park, Lee Soon;Lee, Tae Hyung;Kim, Soon Hak;Chang, Jin Gyu
    • Applied Chemistry for Engineering
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    • v.10 no.3
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    • pp.427-431
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    • 1999
  • Copolyester resins for the coil coating process of aluminium and steel strip were synthesized and their thermal properties, molecular weight and solvent solution characteristics were examined. Copolyesters were obtained by two step reactions. The first step was to prepare bishydroxyethyl terephthalate (BHET), bishydroxyneopentyl terephthalate (BHNPT), bishydroxyethyl isophthalate (BHEI), bishydroxyneopentyl sebacate (BHNPS), bishydroxyneopentyl adipicate (BHNPA) and bishydroxyethyl adipicate (BHEA) oligomers by esterification reactions. The second step was the polycondensation reaction utilizing those oligomers to obtain relatively high molecular weight copolyesters (Mw = 30,000~59,000 g/mol) as measured by GPC. These copolyesters were amorphous polymers as shown by DSC without $T_m$ peaks probably due to the kink structure introduced by BHET oligomer and relatively large free volume by bulky BHNPT and BHNPS oligomers. The copolyester samples with half of BHET oligomer substituted by BHNPT while keeping BHEI (0.3 mole) and BHNPS (0.1 mole) ratio constant showed glass transition temperature above $40^{\circ}C$ and good solubility in toluene both at low ($-5^{\circ}C$) temperature and room temperature.

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Kinetic Study on Preparation of Iron Fine Powders by Hydrogen Reduction of Ferous Chloride Vapor (염화물의 기상환원반응에 의한 미립질 철분말의 생성속도에 관한 연구)

  • Lee, Hwa-Yeong;Kim, Seong-Gyu
    • Korean Journal of Materials Research
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    • v.10 no.6
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    • pp.385-391
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    • 2000
  • A kinetic study on the preparation of iron powder by hydrogen reduction of ferrous chloride vapor has been carried out both experimentally and theoretically. For the preparation of iron powder, ferrous chloride was vaporized and transported to a reaction zone by Ar gas used as carrier. Ferrous chloride vapor and hydrogen were mixed and subject to a reduction reaction at high temperature to produce iron powder and HCI gas. Iron powder was collected with organic solvent at the end of reaction zone and HCI gas was also absorbed in a caustic soda solution to determine the conversion ratio of ferrous chloride. For the development of rate equations, a 1st-order reaction and equilibration of ferrous chloride vapor with Ar gas were assumed. According to the results, the rate constant, k could be expressed as $k=7,879exp(-53,840/RT)\textrm{dm}^3/mole.sec$ and the activation energy was found to be 53.84kJ/mole. From TEM observation, the particle size distribution of iron powder produced was found to be in the range of $0.1~1.0{\mu\textrm{m}}$ which was not significantly influenced by reaction temperature or gas flow rates.

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Determination of radiolysis products in Tri-Octyl Amine by high performance liquid chromatography-mass spectrometer (HPLC-MS에 의한 Tri-Octyl Amine(TOA)의 방사선 분해산물 정량)

  • Yang, Han-Beom;Lee, Eil-Hee;Moon, Hyung-Sil
    • Analytical Science and Technology
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    • v.18 no.3
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    • pp.201-205
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    • 2005
  • Tri-octyl amine (TOA) is used in solvent extraction process for radioactive waste. This compound may be degraded to di-octyl amine (DOA), mono-octyl amine (MOA) by radioactive materials. Amount of TOA, DOA and MOA in TOA must be monitored because they production of these compounds means degradation of which leads to a decrease in the extraction yield. Retention behavior for TOA, DOA and MOA are studied with Phenomenex LUNA-$C_{18}$ ($4.6mm{\times}25cm$) analytical column and $CH_3OH:H_2O$ (50 mmol $CH_3COONH_4$) eluent by liquid chromatography. Optimum condition for these compounds is $CH_3OH:H_2O$ (50 mmol $CH_3COONH_4$) = 85 : 15 ratio. TOA, DOA and MOA compounds is well separated within 20 minute. Dynamic range is $30{\sim}160{\mu}g/mL$ for TOA, $5{\sim}100{\mu}g/mL$ for DOA and $0.1{\sim}5{\mu}g/mL$ for MOA, respectively. The detection limit are $0.1{\mu}g/mL$ for TOA, $1{\mu}g/mL$ for DOA (in SCAN mode) and $0.1{\mu}g/mL$ for MOA (in SIM mode) in this system with $20{\mu}L$ sample loop.

Preparation of Pelletized Porous Adsorbent with Pyrolysis Temperature and Its Toluene Gas Adsorption Characteristics (열분해 조건에 따른 펠렛형 다공성 흡착재의 제조 및 톨루엔 가스 흡착 특성)

  • Kim, Do Young;Kim, Yesol;Cho, Seho;Jung, Jin-Young;Kim, Min Il;Lee, Young-Seak
    • Applied Chemistry for Engineering
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    • v.24 no.6
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    • pp.587-592
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    • 2013
  • In this study, we prepared pelletized porous carbon adsorbent (PCA) according to the different pyrolysis temperature using activated carbon and polyvinyl alcohol (PVA) as a binder for the removal of toluene, which is one of the representative volatile organic compounds (VOCs). We investigated physical characteristics of PCA using FE-SEM, BET, TGA and evaluated their adsorption capacity for toluene using GC. It was confirmed that the formability of pellets composed of the activated carbon, PVA and solvent of mass mixing ratio was 1 : 0.2 : 0.8 was the most outstanding. Toluene adsorption capacity was evaluated by measuring the maximum time when more than 99% of toluene adsorbed on the pellet. The specific surface area of the adsorbent pyrolyzed at $300^{\circ}C$ was measured as 4.7 times in $941.9m^2/g$ compared to that of the unpyrolyzed pellet. Micropore volume and toluene adsorption capacity of PCA increased fivefold to be 0.30 cc/g and thirteenfold to be 26 hours compared to that of the unpyrolyzed pellet, respectively. These results were attributed to the change of pore size and specific surface area due to the PVA content and the different pyrolysis temperature.

Correlation of Antioxidant and Antimutagenic Activity with Content of Pigments and Phenolic Compounds of Colored Rice Seeds (유색미 색소체 및 페놀성화합물 함량과 항산화.항변이원성 간의 상관관계)

  • Kang, Mi-Young;Shin, Soo-Young;Nam, Seok-Hyun
    • Korean Journal of Food Science and Technology
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    • v.35 no.5
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    • pp.968-974
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    • 2003
  • Twenty-three cultivars of colored rice were collected from inside and outside Korea to determine the contents of pigments and phenolic compounds, and also to compare their correlations with antioxidativity and antimutagenicity. The pigment content decreased in the order of LK 1-3-6-12-1-1>LK 1D 2-7-12-1-1>Elwee>Mutumanikam>IR 1544-38-2-2-1-2-2>wx 124-163-45-7-1-1-1, LK 1A-2-12-1-1. Polyphenolic content was the greatest in IR 17491-5-4-3-3 with a ratio of 0.244 g per 100 g brown rice, followed by LK 1-3-6-12-1-1>LK 1D2-12-1>Elwee>Mutumanikam 7 IR 1544-38-2-2-1-2-2, LK 1A-2-12-1-1. The pigment contents for each colored rice cultivar showed a highly positive correlation with polyphenolics in colored rice seeds. For chromaticity, a positive correlation was exhibited between the lightness and hydroxyl radical scavenging activity. In contrast, a negative correlation was observed between the redness and the inhibitory effect of lipid peroxidation.

Chemical Component, Antioxidative and Antimicrobial Activities of Chestnut(Castanea crenata) Leaves (밤나무 잎의 화학성분, 항산화 및 항균활성)

  • 정창호;허재연;심기환
    • Food Science and Preservation
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    • v.9 no.2
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    • pp.234-239
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    • 2002
  • To study the potential of the chestnut(Castanea crenata S.) leaves, as raw materials for functional food and medicine, chemical components, antioxidative and antimicrobial activities were carried out. The proximate composition was composed of total sugar 11.95%, crude fat 11.50%, crude fiber 10.11%, crude protein 7.50% and ash 1.79% and the components of major minerals were Ca 215.7 mg%, 196.6 mg%. The content of vitamin C wag 12.5 mg% and free sugar was composed of glucose 3.33%, fructose 0.25% and sucrose 0.022%. The major fatty acids in leaves of chestnut were composed of linoleic acid and the amounts of those showed 37.88% area percent. The major amino acids of chestnut leaves were glutamic acid(295.4 mg%), proline(285.7 mg%), aspartic acid(245.5 mg%), arginine(240.8 mg%), phenylalanine(237.4 mg%) and leucine(230.6 mg%). The ratio of essential/total amino acid was 48.3%. Methanol extract and ethyl acetate fraction showed stronger activity of the hydrogen donating activities, each of 72.52 % and 84.12 %, respectively. In solvent extracts using methanol, ethanol, ethyl acetate, chloroform and hexane, methanol extract showed the most effective antimicrobial activities. Antimicrobial activities of ethyl acetate fraction of methanol extract was higher than those of other fractions.

Preparation and Release Behavior of Atorvastatin Calcuim - Encapsulated Polyoxalate Microspheres (아토르바스타틴 칼슘을 함유한 폴리옥살레이트 미립구의 제조 및 방출거동)

  • Lee, Cheon Jung;Kim, Su Young;Lee, Hyun Gu;Yang, Jaewon;Park, Jin Young;Cha, Se Rom;Lim, Dong-Kwon;Lee, Dongwon;Khang, Gilson
    • Polymer(Korea)
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    • v.38 no.5
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    • pp.656-663
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    • 2014
  • Atorvastatin calcium-loaded polyoxalate (POX) microspheres were prepared by an emulsion solvent-evaporation/ extraction method of oil-in-oil-in-water ($O_1/O_2/W$) for sustained release. We investigated the release behavior according to initial drug ratio, molecular weight ($M_w$) and concentration of POX and concentration of emulsifier. The microsphere was characterized on the surface, the cross-section morphology and the behavior of atorvastatin calcium release for 10 days by scanning electron microscopy (SEM) and high performance liquid chromatography (HPLC). The analysis of crystallization was analyzed to use X-ray diffraction (XRD), differential scanning calorimeter (DSC) and Fourier transform infrared (FTIR). These results showed that the release behaviors can be controlled by preparation conditions.

Competitive Extraction of Chlorinated Solvents by Headspace SPME GC/FID (Headspace SPME GC/FID를 이용한 Chlorinated Solvents의 경쟁적 추출효과에 관한 연구)

  • An, Sangwoo;Kim, Youngju;Chun, Sukyoung;Lee, Sijin;Park, Jaewoo;Chang, Soonwoong
    • Journal of the Korean GEO-environmental Society
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    • v.11 no.5
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    • pp.61-67
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    • 2010
  • In this study, Solid-phase microextraction (SPME) with GC/FID was studied as a possible alternative to liquid-liquid extraction for the analysis of chlorinated solvents (PCE and TCE) and these by-products (cis-DCE, VC, and Ethylene). Experimental parameters affecting the SPME process (such as kind of fibers, adsorption time, desorption time, volume ratio of sample to headspace, salt addition, and magnetic stirring) were optimized. Experimental parameters such as CAR/PDMS, adsorption time of 20 min, desorption time of 5 min at $250^{\circ}C$, headspace volume of 50mL, sodium chloride (NaCl) concentration of 25% combined with magnetic stirring were selected in optimal experimental conditions for analysis of chlorinated solvents and these by-products. The general affinity of analytes to CAR/PDMS fiber was high in the order PCE>TCE>cis-DCE>VC>Ethylene. The linearity of $R^2$ for chlorinated solvents and these by-products was from 0.912 to 0.999 when analyte concentrations range from $10{\mu}g/L$ to $500{\mu}g/L$, respectively. The relative standard deviation (% RSD) were from 2.1% to 3.6% for concentration of $500{\mu}g/L$ (n=5), respectively. Finally, the limited of detection (LOD) observed in our study for chlorinated solvents and these by-products were from $0.5{\mu}g/L$ to $10{\mu}g/L$, respectively.

Extraction of Carbohydrates and Minerals from Laminaria Using Organic Acid (다시마 뿌리로부터 유기산을 이용한 다당과 미네랄 추출)

  • Chun, Ji Yeon;Han, Cha Seong;Lee, Jung Shik;Kim, Young Suk;Park, Kwon Pil
    • Korean Chemical Engineering Research
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    • v.50 no.2
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    • pp.238-243
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    • 2012
  • Laminaria roots have not been practically used in Korea. In this study, the extraction process of carbohydrates and minerals from Laminaria roots was investigated and the properties of extracted components were measured. Hydrochloric acid generally used in carbohydrate extraction from seaweeds in order to obtain high extraction yield. But in this work, to utilize extracted components as a functional food material, organic acids such as citric acid were used. Organic acid as extraction solvent has low extraction yield compared to strong acids. Therefore optimum condition for maximum yield was investigated in carbohydrate extraction from Laminaria roots using organic acid. We measured the extraction yields of carbohydrate with variation of extraction temperature, extraction time, concentration of organic acid and particle size of samples. The extraction yield increased as the particle size decreased and temperature became high. The extraction yield was 19.0 wt% after 4.0 hours extraction with 0.2 wt% citric acid at $100^{\circ}C$. Potassium concentration was high compared other minerals in extraction solution, that is, the ratio of K/Na was about 3.0. Fucoidan from Laminaria roots had same carbohydrate composition and lower molecular weight compared that of Undaria pinnatifida.